AU2020102823A4 - Method for preparing carbon nanotube-porous carbon composite materials - Google Patents
Method for preparing carbon nanotube-porous carbon composite materials Download PDFInfo
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- AU2020102823A4 AU2020102823A4 AU2020102823A AU2020102823A AU2020102823A4 AU 2020102823 A4 AU2020102823 A4 AU 2020102823A4 AU 2020102823 A AU2020102823 A AU 2020102823A AU 2020102823 A AU2020102823 A AU 2020102823A AU 2020102823 A4 AU2020102823 A4 AU 2020102823A4
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
Abstract
The disclosure relates to a method for preparing a carbon nanotube-porous carbon
composite material, comprising the following steps: firstly dispersing lamellar
porous magnesium oxide in water to obtain suspension, then dropwise adding nickel
nitrate solution into the suspension, filtering in vacuum after evenly mixing, drying
filter residues, smashing, calcining to obtain a carbon tube template, adding the
carbon tube template and a carbon precursor into a solvent in a weight ratio of
(0.5~10):1, evenly mixing and then drying, then calcining at high temperature under
a protective gas, cooling and taking out to obtain black powder, acid picking, then
rinsing with deionized water to be neutral, finally, filtering in vacuum, and drying.
The method is simple to operate, low in cost, beneficial to batch production on large
scale, and can realize the synchronous regulation and control of the morphology and
structure of the carbon nanotube-porous carbon composite material. The prepared
composite material remains the lamellar morphology of the template, has mesopore
micropore hierarchical pore distribution, is high in conductivity and rich in pore
structure, and can be used in the fields of energy storage, catalysis and the like as an
electrode material, a catalytic material or a catalyst carrier.
1/6
DRAWINGS
FIG. 1
700
600
500
400
-3 300
o 200
100
0
0
-100 1 , , , i , ,
0.0 0.2 0.4 0.6 0.8 1.0
Relative pressure (P/Po)
FIG. 2
Description
1/6
FIG. 1
700
600
500
400
-3 300
o 200
100 0 0
-100 1 , , , i , ,
0.0 0.2 0.4 0.6 0.8 1.0 Relative pressure (P/Po)
FIG. 2
[0001] The disclosure relates to a method for preparing carbon nanotube-porous carbon composite materials, belonging to the technical field of carbon materials.
[0002] Carbon nanotube-porous carbon composite materials are porous nano carbon materials containing 3D network structure, which not only has rich pore structures but also has conductivity provided by conductive networks of carbon nanotubes. Compared with pure porous carbons, the carbon nanotube-porous carbon composite materials has a firmer bulk phase structure and a faster electron transmission rate, and have wide application prospect in the fields of energy storage, optoelectronic, catalysis.
[0003] The objective of the disclosure is to solve the deficiency of the methods for preparing carbon nanotube-porous carbon composite materials in the existing technology and provides a simple method for preparing carbon nanotube-porous carbon composite materials. The method does not need to pre-disperse the carbon nanotubes in advance, which is simple to operate, low in cost and conducive to large scale production. In particular, this method can realize the synchronous regulation and control of the morphology and structure of the carbon nanotube-porous carbon composite material. The prepared carbon nanotube-porous carbon composite material has the advantages of both high conductivity and porous structure.
Technical solution
[0004] The disclosure adopts a carbon precursor which is low in cost, realizes one-step preparation of a carbon nanotube-porous carbon composite material by template method. Coating on the template is realized during the calcination process, with the help of the high-temperature fluidity of the carbon precursor, solving the drawbacks of existing preparation of carbon nanotube-porous carbon composite materials with a two-step method, and can realize the synchronous regulation and control of the morphology and structure of the carbon nanotube-porous carbon composite material. Special solution is as follows:
[0005] A method for preparing a carbon nanotube-porous carbon composite material, comprising the following steps:
[0006] (1) dispersing lamellar porous magnesium oxide in water to obtain suspension, then dropwise adding nickel nitrate solution into the suspension, filtering in vacuum after evenly mixing, drying filter residues, smashing, and calcining to obtain a carbon tube template;
[0007] (2) adding the carbon tube template and a carbon precursor into a solvent in a weight ratio of (0.5~10):1, stirring, evenly mixing and then drying, then calcining the obtained powder for 5-90 min at high temperature under a protective gas, cooling and taking out to obtain black powder, carrying out acid picking on the black powder, then rinsing with deionized water to be neutral, finally, filtering in vacuum, and drying to obtain the carbon nanotube-porous carbon composite material;
[0008] in step (2), the carbon precursor being selected from one of pitch, coal tar, vacuum residuum or oil slurry.
[0009] Further, in step (1), a method for preparing lamellar porous magnesium oxide comprises: 30g of light magnesium oxide is added into 300 mL of water, boiled with water and refluxed for 24 h, cooled, filtered in vacuum and dried, the filter cake obtained by drying is smashed and calcined for 1 h at 550°C, so as to obtain lamellar porous magnesium oxide.
[0010] Further, in step (1), the mass concentration of suspension is 100g/L.
[0011] Further, in step (1), a mass ratio of lamellar porous magnesium oxide to nickel nitrate is 10:0.63.
[0012] Further, in step (1), the calcination temperature is 550°C, and the time is 30 min.
[0013] The disclosure has the beneficial effects that: the disclosure adopts a low-cost carbon precursor, realizes the one-step preparation of the carbon nanotube porous carbon composite material by utilizing the high-temperature fluidity of the carbon precursor itself by virtue of the template method. The method does not need to evenly disperse the carbon nanotubes in advance, is simple to operate, low in cost and beneficial to batch production on large scale, and can realize the synchronous regulation and control of the morphology and structure of the carbon nanotube-porous carbon composite material. The prepared carbon nanotube-porous carbon composite material remains the lamellar morphology of the template, has a specific surface area of 500-1000 m2 -1, has mesopore-micropore hierarchical pore distribution, has the advantages of high conductivity, rich pore structure and the like, and can be used in the fields of energy storage, catalysis and the like as an electrode material, a catalytic material or a catalyst carrier.
[0014] Fig.1 is a transmission electron micrograph of a carbon nanotube-porous carbon composite material prepared in example 1.
[0015] Fig.2 shows adsorption and desorption curves of a carbon nanotube-porous carbon composite material prepared in example 1.
[0016] Fig.3 shows a pore size distribution curve of a carbon nanotube-porous carbon composite material prepared in example 1.
[0017] Fig.4 is a Raman spectrogram of a carbon nanotube-porous carbon composite material prepared in example 1.
[0018] Fig. 5 is a scanning electron micrograph of a porous carbon material prepared in example 1.
[0019] Fig.6 shows adsorption and desorption curves of a porous carbon material prepared in example 1.
[0020] Fig. 7 shows a pore size distribution curve of a porous carbon material prepared in example 1.
[0021] Fig. 8 shows CV curves of a carbon nanotube-porous carbon composite material in example 1 and a porous material prepared in comparative example 1 (a scanning speed is 100 mV s-1).
[0022] Fig. 9 is a transmission electron micrograph of a carbon nanotube-porous carbon composite material prepared in example 2.
[0023] Fig. 10 shows adsorption and desorption curves of a carbon nanotube-porous carbon composite material prepared in example 2.
[0024] Fig. 11 shows a pore size distribution curve of a carbon nanotube-porous carbon composite material prepared in example 2.
[0025] Fig. 12 is a Raman spectrogram of a carbon nanotube-porous carbon composite material prepared in example 2.
[0026] The disclosure will be further described in combination with drawings and embodiments.
[0027] In the following examples, a method for preparing lamellar porous magnesium oxide comprises: 30g of light magnesium oxide is added into 300 mL of water, boiled with water and refluxed for 24 h, cooled, filtered in vacuum and dried, and the filter cake obtained by drying is smashed and calcined for 1 h at 550°C, so as to obtain lamellar porous magnesium oxide.
Example 1
[0028] A method for preparing a carbon nanotube-porous carbon composite material comprises the following steps:
[0029] (1) 1Og of lamellar porous magnesium oxide was dispersed into water to obtain suspension, then nickel nitrate solution (0.63g of nickel nitrate was dissolved into 8mL of water) was dropwise added into the suspension, the mixed solution was subjected to ultrasound treatment for 30 min to be evenly mixed, and then suction filtration was carried out, the obtained filter residue was dried and then smashed, and subsequently calcined for 30 min at 550 °C to obtain a carbon tube template;
[0030] (2) 1Og of carbon tube template and 1Og of pitch were added into solvent ethanol and then stirred, evenly mixed and dried, the obtained powder was placed in ceramic boat, calcined for 30 min at 800°C under the protection of nitrogen gas in a high-temperature tube furnace, the calcined powder was cooled and taken out to obtain black powder, the black powder was subjected to acid picking with diluted hydrochloric acid, then rinsed with deionized water to be neutral, finally, filtered in vacuum and dried to obtain the carbon nanotube-porous carbon composite material. The yield was %. The specific surface area was measured as 1001.4 m 2/g.
[0031] The transmission electron micrograph of the carbon nanotube-porous carbon composite material prepared in example 1 is shown in Fig.1. It can be seen from Fig.1 that a large number of carbon nanotubes are evenly intertweaved in the carbon layer to form a network structure.
[0032] The adsorption and desorption curves of the carbon nanotube-porous carbon composite material prepared in example 1 are shown in Fig.2, and the pore size distribution curve is shown in Fig.3. It can be seen that the prepared carbon nanotube-porous carbon composite material has micropores and mesopores, and the desorption pore sizes distribution is in 2.5~4.5 nm.
[0033] The Raman spectrogram of the carbon nanotube-porous carbon composite material prepared in example 1 is shown in Fig.4. The higher D peak in Fig.4 indicates that there are lots of defect positions, and the sharp G peak is donated by graphitization of the carbon layer and the carbon nanotubes.
Comparative example 1
[0034] Preparation method of a porous carbon material: 10 g of lamellar porous magnesium oxide template and 10 g of pitch were magnetically stirred and evenly mixed in ethanol, and then dried in forced air in an oven of 80 °C to obtain gray powder. The powder was put in a ceramic boat and calcined for 30 min at 800 °C under the protection of a nitrogen gas in a high temperature horizontal tube furnace, then the calcined powder was cooled and taken out, the obtained powder was subjected to acid pickling with diluted hydrochloric acid to remove the template, and then the powder without the template was washed with deionized water to be neutral, filtered in vacuum and dried to obtain a black powder porous carbon material. The yield was 48%. The specific surface area was measured as 761.8 m2/g.
[0035] The scanning electron micrograph of the porous carbon material prepared in comparative example 1is shown in Fig. 5. It can be seen that the porous carbon has the lamellar morphology of the template. The adsorption and desorption curves of the porous carbon material are shown in Fig. 6 and the pore size distribution curve is shown in Fig. 7. It can be seen that the pore size distribution of the porous carbon material is wide, which is in 3-5.5 nm.
[0036] The CV curves of the carbon nanotube-porous carbon composite material in example 1 and the porous carbon material in comparative example 1 are shown in Fig.
8. It can be seen that compared with the porous carbon material in comparative example 1, the CV curve of the material obtained in example 1 at a scanning speed of 100 mV-s-1 is of a more standard rectangle, indicating that after carbon and nano tubes are composited, the conductivity of this material is obviously improved, the pore structure is more rich, and specific capacity is increased.
Example 2
[0037] A method for preparing a carbon nanotube-porous carbon composite material comprises the following steps:
[0038] (1) the preparation of the carbon template was the same as that in example 1;
[0039] (2) 1Og of carbon tube template and 1Og of pitch into solvent ethanol, stirred and evenly mixed and dried, the obtained powder was placed in a ceramic boat, calcined for 20 min at 900°C under the protection of a nitrogen gas in a high-temperature tube furnace, the calcined powder was cooled and taken out to obtain black powder, the black powder was subjected to acid picking with diluted hydrochloric acid, then rinsed with deionized water to be neutral, finally filtered in vacuum and dried to obtain the carbon nanotube-porous carbon composite material. The specific surface area was measured as 984.6 m2.
[0040] The transmission electron micrograph of the carbon nanotube-porous carbon composite material prepared in example 2 is shown in Fig.9. It can be seen from Fig.9 that a large number of carbon nanotubes are evenly intertweaved in the carbon layer to form a network structure.
[0041] The adsorption and desorption curves of the carbon nanotube-porous carbon composite material prepared in example 2 are shown in Fig.10, and the pore size distribution is shown in Fig.11. It can be seen that the prepared carbon nanotube-porous carbon composite material has micropores and mesopores, and the desorption pore size distribution is in 2.5-5 nm.
[0042] The Raman spectrogram of the carbon nanotube-porous carbon composite material prepared in example 2 is shown in Fig.12. In Fig.12, the D peak and the G peak respectively represent the defect position and graphitization degree of the composite material.
Claims (5)
1. A method for preparing a carbon nanotube-porous carbon composite material, comprising the following steps:
(1) dispersing lamellar porous magnesium oxide in water to obtain suspension, then dropwise adding nickel nitrate solution into the suspension, filtering in vacuum after evenly mixing, drying filter residues, smashing, and calcining to obtain a carbon tube template; (2) adding the carbon tube template and a carbon precursor into a solvent in a weight ratio of (0.5~10):1, evenly mixing and then drying, calcining the obtained powder for 5-90 min at high temperature under a protective gas, cooling and taking out to obtain black powder, acid picking, then rinsing with deionized water to be neutral, finally, filtering in vacuum, and drying to obtain the carbon nanotube-porous carbon composite material; in step (2), the carbon precursor being selected from one of pitch, coal tar, vacuum residuum or oil slurry.
2. The method for preparing the carbon nanotube-porous carbon composite material according to claim 1, wherein in step (1), a method for preparing lamellar porous magnesium oxide comprises: 30g of light magnesium oxide is added into 300 mL of water, boiled with water and refluxed for 24 h, cooled, filtered in vacuum and dried, the filter cake obtained by drying is smashed, and the smashed filter cake is calcined for 1 h at 550°C, so as to obtain lamellar porous magnesium oxide.
3. The method for preparing the carbon nanotube-porous carbon composite material according to claim 1, wherein in step (1), the mass concentration of suspension is 100g/L.
4. The method for preparing the carbon nanotube-porous carbon composite material according to claim 1, wherein in step (1), a mass ratio of lamellar porous magnesium oxide to nickel nitrate is 10:0.63.
5. The method for preparing the carbon nanotube-porous carbon composite material according to claim 1, wherein in step (1), the calcination temperature is 550°C, and the time is 30 min.
Adsorption capacity (cm3/g) DRAWINGS 1/6
FIG. 2 FIG. 1
Relative pressure (P/P0)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114883117A (en) * | 2021-05-17 | 2022-08-09 | 安徽科技学院 | Preparation method of composite carbon nano tube |
| CN114933294A (en) * | 2022-05-13 | 2022-08-23 | 西安交通大学 | High-volume-density multilayer compact porous carbon nanosheet and preparation method and application thereof |
| CN115331978A (en) * | 2022-09-02 | 2022-11-11 | 河北工业大学 | Preparation method and application of positive and negative electrode matching material of lithium ion hybrid capacitor |
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2020
- 2020-10-16 AU AU2020102823A patent/AU2020102823A4/en not_active Ceased
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114883117A (en) * | 2021-05-17 | 2022-08-09 | 安徽科技学院 | Preparation method of composite carbon nano tube |
| CN114883117B (en) * | 2021-05-17 | 2023-04-21 | 安徽科技学院 | Preparation method of composite carbon nano tube |
| CN114933294A (en) * | 2022-05-13 | 2022-08-23 | 西安交通大学 | High-volume-density multilayer compact porous carbon nanosheet and preparation method and application thereof |
| CN115331978A (en) * | 2022-09-02 | 2022-11-11 | 河北工业大学 | Preparation method and application of positive and negative electrode matching material of lithium ion hybrid capacitor |
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